Ni-Fe/La2O3 catalyst prepared by a glow discharge plasma treatment following calcinations thermally exhibits higher activity and selectivity compared to the Ni-Fe/La2O3 prepared conventionally. At the same reaction temperature, the CH4 conversion, CO selectivity and H-2 selectivity obtained from the plasma prepared Ni-Fe/La2O3 are 5-9%,4-7% and 9-15% higher than those from the conventional Ni-Fe/La2O3 catalyst, respectively. At the same methane conversion, the reaction temperature with the plasma prepared Ni-Fe/La2O3 is at least 100degreesC lower than that with the conventional Ni-Fe/La2O3.